HCID 44220043, compound → HCID 44220233, compound

Participants

Reaction Steps

Two drops of CF3SO3H was added to a flask containing 80 mg 6a and 2 mL CH2Cl2 at RT, and the mixture was stirred for about 2 h (monitored by TLC). The mixture was purified directly by column chromatograph to obtain 7 as a white solid (78%): mp 165-167° C., 1H NMR, δ 2.78-2.84 (dd, J=8.1 & 4.2 Hz, 2H), 3.16-3.22 (dd, J=8.1 & 4.2 Hz, 2H), 3.92 (s, 3H), 7.19-7.34 (m, 6H), 9.34 (s, 1H); 13C NMR, δ 28.38, 37.49, 52.12, 118.81 (m), 122.02 (m), 126.19, 128.00 (m), 128.58, 128.61, 138.50 (m), 142.07, 161.26; 19F NMR, δ 88.87 (p, J=148 Hz, 1H), 73.56 (d, J=148 Hz, 4H); HRMS, calc for C14H14F5NO2S, 355.0665; found, 355.0648; Anal, calc for C14H14F5NO2S: C, 47.32; H, 3.97; N, 3.94; found: C, 47.04; H, 3.68; N, 3.86.

Provenance & Evidence